CN103884571A - Method for testing content of magnetic substances in lithium ion battery anode material - Google Patents
Method for testing content of magnetic substances in lithium ion battery anode material Download PDFInfo
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Abstract
The invention discloses a method for testing the content of magnetic substances in a lithium ion battery anode material. The method comprises the following steps: ultrasonically dispersing a lithium ion battery anode material to be tested into a solvent, adding a polymer cladded magnet, ultrasonically adsorbing the magnetic substances, thereby obtaining the polymer cladded magnet adsorbed with the magnetic substances; adding the polymer cladded magnet adsorbed with the magnetic substances into a cleaning solution for performing ultrasonic cleaning; dissolving the cleaned polymer cladded magnet adsorbed with the magnetic substances by using an acidic reagent, thereby obtaining a dissolution solution; and testing the content of the magnetic substances in the dissolution solution. According to the method, the content of the magnetic substances in the lithium ion battery anode material can be accurately tested, particularly the content of the magnetic substances contained in micron order materials and nanoscale materials can be accurately detected. The testing method is simple, easy to operate and high in precision, and the precision can reach a ppb level.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, especially relate to the method for testing of magnetisable material content in a kind of anode material for lithium-ion batteries.
Background technology
It is high that lithium ion battery has energy density, and many good characteristics such as good cycle, have been widely used in the aspects such as portable type electronic product, communication tool, electric automobile and energy storage device.The market of rapid growth has proposed an urgent demand of high power capacity, long-life, high security to lithium ion battery, the raising of performance of lithium ion battery becomes the key of industry development, and positive electrode is depended in the performance of performance of lithium ion battery to a great extent.
In recent years, research is found to contain magnetic metal impurity in anode material for lithium-ion batteries, the existence of these magnetisable materials, not only can reduce specific storage and the energy density of material, and some magnetic impurity is soluble in electrolytic solution, there are a series of subsidiary reactions, cause serviceable life, consistance and the security performance of battery to reduce.In anode material for lithium-ion batteries, magnetisable material also has direct impact to self-discharge of battery, and magnetisable material content is directly proportional to self-discharge of battery rate, i.e. the higher positive electrode of magnetisable material content, and the self-discharge rate of the battery of its composition is larger.
Therefore, how accurately detecting magnetisable material content in anode material for lithium-ion batteries is lithium ion battery circle urgent problem.
Application number is the detection method that 2010101663831 patent of invention discloses a kind of magnetic substances in powder material of lithium ion battery, after fully being stirred together with magnet, powder body material takes out magnet, take out the powder body material adsorbing on magnet, clean magnet with acid solution afterwards and obtain cleaning fluid, detect the magnetisable material in cleaning fluid.The method is directly used the magnetisable material in magnet adsorption material, exist magnetisable material that magnetisable material can not be adsorbed or be adsorbed completely because of the coated nonmagnetic substance of skin be cleaned may, thereby cause accuracy of detection not high, poor for applicability while particularly testing nano material, and in lithium ion battery material, have a lot of nano materials at present.
Summary of the invention
In view of above the deficiencies in the prior art, the invention provides the method for testing of magnetisable material content in high, the easy to operate anode material for lithium-ion batteries of a kind of accuracy of detection.
The present invention is achieved in that the method for testing of magnetisable material content in a kind of anode material for lithium-ion batteries, comprises the following steps:
Be scattered in solvent ultrasonic anode material for lithium-ion batteries to be tested, then add polymer overmold magnet, ultrasonic absorption magnetisable material, obtains the polymer overmold magnet that adsorbs the material that is magnetic;
The be magnetic polymer overmold magnet of material of described absorption is added and in cleaning fluid, carries out ultrasonic cleaning;
The polymer overmold magnet that dissolves the absorption magnetisable material after cleaning with acid reagent, obtains lysate;
Test the magnetisable material content in described lysate.
The method of testing of magnetisable material content in anode material for lithium-ion batteries of the present invention, can accurately test the content of magnetisable material in anode material for lithium-ion batteries, especially can accurately detect the content in micron order material and nanometer materials with magnetisable material, method of testing of the present invention is simple to operation, precision is high, can be accurate to ppb level.
Embodiment
In order to make technical matters to be solved by this invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The method of testing of magnetisable material content in embodiment of the present invention anode material for lithium-ion batteries, comprises the following steps:
S1: be scattered in solvent ultrasonic anode material for lithium-ion batteries to be tested, form finely dispersed solution;
S2: add polymer overmold magnet, the magnetisable material in ultrasonic adsorbent solution, obtains the polymer overmold magnet that adsorbs the material that is magnetic again;
S3: the be magnetic polymer overmold magnet of material of absorption is added and carries out ultrasonic cleaning in cleaning fluid;
S4: dissolve and clean the magnetisable material adsorbing on rear magnet with acid reagent, obtain lysate and obtain solution to be measured after core filtration unit filters;
S5: adopt magnetisable material content in the above-mentioned solution to be measured of icp ms test.
Particularly, the frequency of ultrasonic dispersion described in step S1 is 20-100kHz, and the processing time is 10-100min; Testing sample is added to and in solvent, carries out ultrasonic processing, the magnetisable material of cluster of grains aggressiveness inside in testing sample is dispersed in solvent by ultrasonic method, so that all magnetisable materials are fully adsorbed by magnet in sample, avoid, because magnetisable material cannot be adsorbed because magnetic weakens after being coated by sample, affecting test result accuracy.The solvent that adopts is selected from a kind of in ethanol, deionized water, acetone, isopropyl alcohol or ethane diacid or more than one potpourri.
In step S2, the frequency of described ultrasonic absorption is 20-100kHz, and the processing time is 10-30min; The intensity of magnet is preferably 3000-12000 Gauss, more preferably 6000 Gausses.Magnet surface is coated with polymkeric substance, avoids introducing new impurity, affects test result precision, preferably scribbles the coated magnet of PTFE anti-wear layer.
In step S3, cleaning fluid is selected from a kind of in ethanol, deionized water, acetone, isopropyl alcohol or ethane diacid or more than one potpourri.The frequency of ultrasonic cleaning is 20-100kHz, and the processing time is 10-30min; Remove the non-magnetic material on magnet by carrying out ultrasonic cleaning in the abundant magnet input cleaning fluid that adsorbs the material that is magnetic in step S2.Change the cleaning fluid in container, repeating step S3 until ultrasonic rear cleaning fluid be colourless and there is no suspension.
In step S4, the mixed solution of the preferred hydrochloric acid of acid reagent and nitric acid, fully dissolves the magnetisable material on magnet.In course of dissolution, can further heat and promote to dissolve, as adopted electrothermal furnace to be heated to keep 15-60min after micro-boiling, after magnetisable material on magnet dissolves completely, use deionized water rinsing magnet to lysate.With core filtration unit filtration lysate, then repeatedly wash with deionized water, filtrate in filter flask is shifted in volumetric flask, after shaking up, dilution constant volume obtains solution to be measured.
Step S5, adopts inductivity coupled plasma mass spectrometry test magnetisable material content, and measuring accuracy is high.
Magnetisable material comprises: one or more in iron, cobalt, nickel, chromium, copper, zinc, in the building-up process of anode material for lithium-ion batteries, can follow and generate a small amount of magnetisable material impurity, the existence of these impurity can reduce specific storage and the energy density of material, affects serviceable life and the security performance of battery.And the height of self-discharge of battery rate is directly proportional to magnetisable material content, even extremely the magnetisable material of trace also may bring tremendous influence.Magnetisable material method of testing of the present invention is particularly useful for detecting the battery material such as micron order and nanoscale, and accuracy of detection is high, is accurate to ppb level.
Further illustrate below in conjunction with specific embodiment.
Instrument: ultrasonic separating apparatus (40kHz), coated magnet (the diameter 2cm of teflon, height 8cm, 6000 Gausses), core filtration unit, analytical balance (being accurate to 0.0001g), volumetric flask, inductivity coupled plasma mass spectrometry (ICP-MS2000)
Reagent: absolute ethyl alcohol, hydrochloric acid (15wt%), nitric acid (30wt%), mark stock solution, deionized water
Embodiment 1
Take anode material for lithium-ion batteries 100g(LiFePO4 sample) be placed in high-temperature resistance plastice bottle, inject 100g absolute ethyl alcohol, add sealing of lid, bottle is put into the ultrasonic 60min of ultrasonic separating apparatus.
In bottle, add magnet, continue ultrasonic 30min, take out magnet and put into the clean beaker that fills ethanolic solution, after ultrasonic 10 minutes, change the ethanolic solution in beaker, repeat this step, until in ultrasonic rear beaker, ethanolic solution is colourless, and till no suspended substance.
Take out magnet, put into clean beaker, add 20ml salpeter solution and 10ml hydrochloric acid solution, keep 15 minutes, until the magnetisable material on magnet dissolves completely, using deionized water rinsing magnet, to lysate after micro-boiling as for being heated on electrothermal furnace.With core filtration unit filtration lysate, then, with after deionized water washing 5 times, filtrate in filter flask is transferred in 250ml volumetric flask, be diluted to scale, after shaking up, obtain solution to be measured.
Debug icp ms, solution to be measured and standard solution have been tested simultaneously.The magnetisable material that experiment records in sample comprises: iron 12ppb, cobalt 5ppb, nickel 1ppb, chromium 2ppb, copper 2ppb, zinc 1ppb.Magnetisable material content is the summation of the content of iron, cobalt, nickel, chromium, copper, zinc; , magnetisable material content=12+5+1+2+2+1=23ppb
Embodiment 2
Take anode material for lithium-ion batteries 100g(cobalt acid lithium sample) be placed in high-temperature resistance plastice bottle, inject 100g isopropyl alcohol, add sealing of lid, bottle is put into the ultrasonic 30min of ultrasonic separating apparatus.
In bottle, add magnet, continue ultrasonic 40min, take out magnet and put into the clean beaker that fills aqueous isopropanol, after ultrasonic 10 minutes, change the aqueous isopropanol in beaker, repeat this step, until in ultrasonic rear beaker, aqueous isopropanol is colourless, and till no suspended substance.
Take out magnet, put into clean beaker, add 15ml salpeter solution and 10ml hydrochloric acid solution, keep 20 minutes, until the magnetisable material on magnet dissolves completely, using deionized water rinsing magnet, to lysate after micro-boiling as for being heated on electrothermal furnace.With core filtration unit filtration lysate, then, with after deionized water washing 4 times, filtrate in filter flask is transferred in 250ml volumetric flask, be diluted to scale, after shaking up, obtain solution to be measured.
Debug icp ms, solution to be measured and standard solution have been tested simultaneously.The magnetisable material that experiment records in sample comprises: iron 6ppb, cobalt 16ppb, nickel 8ppb, chromium 5ppb, copper 3ppb, zinc 5ppb.Magnetisable material content is the summation of the content of iron, cobalt, nickel, chromium, copper, zinc; , magnetisable material content=6+16+8+5+3+5=43ppb.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a method of testing for magnetisable material content in anode material for lithium-ion batteries, is characterized in that, comprises the following steps:
Be scattered in solvent ultrasonic anode material for lithium-ion batteries to be tested, then add polymer overmold magnet, ultrasonic absorption magnetisable material, obtains the polymer overmold magnet that adsorbs the material that is magnetic;
The be magnetic polymer overmold magnet of material of described absorption is added and in cleaning fluid, carries out ultrasonic cleaning;
Dissolve the be magnetic polymer overmold magnet of material of absorption after cleaning with acid reagent, obtain lysate;
Test the magnetisable material content in described lysate.
2. method of testing according to claim 1, is characterized in that, the frequency of described ultrasonic dispersion is 20-100kHz; Processing time is 10-100min.
3. method of testing according to claim 1 and 2, is characterized in that, the frequency of described ultrasonic absorption is 20-100kHz; Processing time is 10-30min.
4. method of testing according to claim 1 and 2, is characterized in that, the frequency of described ultrasonic cleaning is 20-100kHz; Processing time is 10-30min.
5. method of testing according to claim 1, is characterized in that, described in add and in cleaning fluid, carry out that ultrasonic cleaning repeats once or once, till being colourless and no suspended substance to cleaning fluid.
6. method of testing according to claim 1, is characterized in that, described solvent and cleaning fluid are selected from respectively at least one in ethanol, deionized water, acetone, isopropyl alcohol or ethane diacid.
7. method of testing according to claim 1, is characterized in that, described polymer overmold magnet surface is PTFE anti-wear layer; The intensity of described magnet is 3000-12000 Gauss.
8. method of testing according to claim 1, is characterized in that, the hydrochloric acid solution that described acid reagent is 5～38wt% and 5～68wt% salpeter solution are formulated with the volume ratio of 1:0.1～1.
9. method of testing according to claim 1, is characterized in that, the polymer overmold magnet of the absorption magnetisable material after described cleaning is added in acid flux material, is heated to 30～100 DEG C and obtains lysate.
10. method of testing according to claim 1, is characterized in that, the magnetisable material content measuring in described lysate adopts icp ms.
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| CN106525954A (en) * | 2016-12-21 | 2017-03-22 | 天齐锂业股份有限公司 | Method of detecting magnetic material content in lithium carbonate |
| CN106610352A (en) * | 2015-10-22 | 2017-05-03 | 深圳市比克动力电池有限公司 | Method for detecting magnetic substance content of lithium ion battery positive electrode material |
| CN106770202A (en) * | 2016-12-28 | 2017-05-31 | 彩虹集团新能源股份有限公司 | The assay method of magnetic foreign body content in a kind of energy and material |
| CN106802319A (en) * | 2015-11-26 | 2017-06-06 | 苏州弗莱明磁力技术有限公司 | The detection method of simple substance iron content in a kind of powder |
| CN106802320A (en) * | 2015-11-26 | 2017-06-06 | 苏州弗莱明磁力技术有限公司 | The detection method of simple substance iron content in a kind of powder |
| CN107632012A (en) * | 2017-09-21 | 2018-01-26 | 黄国华 | Determine boron, the method for zr element content in lithium ion battery material |
| CN109314229A (en) * | 2016-06-07 | 2019-02-05 | 住友金属矿山株式会社 | The manufacturing method of lithium compound, the manufacturing method of the lithium compound and non-aqueous electrolyte secondary battery positive active material |
| CN110333168A (en) * | 2019-08-02 | 2019-10-15 | 江苏塔菲尔新能源科技股份有限公司 | A kind of detection method of magnetic-particle |
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| CN110404674A (en) * | 2019-08-08 | 2019-11-05 | 青岛新正锂业有限公司 | The minimizing technology and detection method of magnetisable material in a kind of anode material of lithium battery |
| CN111811984A (en) * | 2020-08-06 | 2020-10-23 | 上海市机电设计研究院有限公司 | Magnetic powder content measuring device |
| CN112179894A (en) * | 2019-07-03 | 2021-01-05 | 万向一二三股份公司 | Method for detecting free iron in lithium iron phosphate anode slurry of lithium ion battery |
| CN112230149A (en) * | 2020-05-25 | 2021-01-15 | 蜂巢能源科技有限公司 | Method for predicting coating falling amount of positive electrode material containing coating |
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| CN115343276A (en) * | 2022-09-02 | 2022-11-15 | 中国电子技术标准化研究院 | Quantitative determination method for magnetic iron foreign matter in lithium iron phosphate for lithium ion battery |
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| CN106610352A (en) * | 2015-10-22 | 2017-05-03 | 深圳市比克动力电池有限公司 | Method for detecting magnetic substance content of lithium ion battery positive electrode material |
| CN106802319A (en) * | 2015-11-26 | 2017-06-06 | 苏州弗莱明磁力技术有限公司 | The detection method of simple substance iron content in a kind of powder |
| CN106802320A (en) * | 2015-11-26 | 2017-06-06 | 苏州弗莱明磁力技术有限公司 | The detection method of simple substance iron content in a kind of powder |
| CN109314229A (en) * | 2016-06-07 | 2019-02-05 | 住友金属矿山株式会社 | The manufacturing method of lithium compound, the manufacturing method of the lithium compound and non-aqueous electrolyte secondary battery positive active material |
| US11056688B2 (en) * | 2016-06-07 | 2021-07-06 | Sumitomo Metal Mining Co., Ltd. | Lithium compound, method for producing the lithium compound, and method for producing positive active material for nonaqueous electrolyte secondary battery |
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| CN109314229B (en) * | 2016-06-07 | 2022-03-01 | 住友金属矿山株式会社 | Lithium compound, method for producing the same, and method for producing positive electrode active material for nonaqueous electrolyte secondary battery |
| CN106525954A (en) * | 2016-12-21 | 2017-03-22 | 天齐锂业股份有限公司 | Method of detecting magnetic material content in lithium carbonate |
| CN106770202A (en) * | 2016-12-28 | 2017-05-31 | 彩虹集团新能源股份有限公司 | The assay method of magnetic foreign body content in a kind of energy and material |
| CN107632012A (en) * | 2017-09-21 | 2018-01-26 | 黄国华 | Determine boron, the method for zr element content in lithium ion battery material |
| CN112179894A (en) * | 2019-07-03 | 2021-01-05 | 万向一二三股份公司 | Method for detecting free iron in lithium iron phosphate anode slurry of lithium ion battery |
| CN110411914A (en) * | 2019-07-30 | 2019-11-05 | 厦门凯纳石墨烯技术股份有限公司 | Lithium ion battery magnetism of material substance detecting method |
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| CN112230149A (en) * | 2020-05-25 | 2021-01-15 | 蜂巢能源科技有限公司 | Method for predicting coating falling amount of positive electrode material containing coating |
| CN111811984A (en) * | 2020-08-06 | 2020-10-23 | 上海市机电设计研究院有限公司 | Magnetic powder content measuring device |
| CN111811984B (en) * | 2020-08-06 | 2022-07-19 | 上海市机电设计研究院有限公司 | Magnetic powder content measuring device |
| CN113376063A (en) * | 2021-05-24 | 2021-09-10 | 合肥国轩高科动力能源有限公司 | Detection method of magnetic foreign matter |
| CN113916965A (en) * | 2021-10-12 | 2022-01-11 | 芜湖天弋能源科技有限公司 | Method for detecting content of magnetic substance in lithium ion battery positive electrode material |
| CN113916965B (en) * | 2021-10-12 | 2023-12-15 | 芜湖天弋能源科技有限公司 | Method for detecting content of magnetic substance in lithium ion battery anode material |
| CN115343276A (en) * | 2022-09-02 | 2022-11-15 | 中国电子技术标准化研究院 | Quantitative determination method for magnetic iron foreign matter in lithium iron phosphate for lithium ion battery |
| CN115343276B (en) * | 2022-09-02 | 2023-08-15 | 中国电子技术标准化研究院 | Quantitative determination method of magnetic iron foreign matters in lithium iron phosphate for lithium ion battery |
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Application publication date: 20140625 |